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尿液中12种苯二氮卓类药物的聚二甲基硅氧烷海绵辅助分散液液微萃取/GC-MS法检测

Determination of 12 Benzodiazepines Drugs in Urine Using Polydimethylsiloxane Sponge-assisted Dispersive Liquid-Liquid Microextraction Coupled with GC-MS

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【作者】 梁未未刘悦林贤文朱焕慧孙立敏陈晓晖王松才

【Author】 LIANG Wei-wei;LIU Yue;LIN Xian-wen;ZHU Huan-hui;SUN Li-min;CHEN Xiao-hui;WANG Song-cai;Guangzhou Institute of Forensic Science;

【通讯作者】 王松才;

【机构】 广州市刑事科学技术研究所

【摘要】 设计了一种基于疏水多孔聚二甲基硅氧烷海绵辅助的分散液液微萃取装置(PDMS-Sponge-DLLME),并实现了对尿液中12种常见苯二氮卓类(BZDs)安眠药的快速高效提取,借助气相色谱-质谱(GC-MS)直接进样完成检验鉴定。通过方糖提供的骨架实现疏水多孔有机PDMS海绵材料的制备,采用傅里叶变换红外光谱、扫描电镜对其微观结构性能进行表征,结合医用注射器、磁搅拌子及橡胶堵头完成该萃取装置的组装,利用内标法进行定量分析。在最优条件下,尿液中12种常见安眠药在0.1~10μg/mL范围内具有良好的线性关系,相关系数(r2)均大于0.99,检出限为0.025~0.200μg/mL,定量下限为0.050~0.400μg/mL,3个加标水平下的回收率为64.4%~112%,相对标准偏差为0.80%~9.4%。该新型分散液液微萃取装置可在数分钟内完成对尿液中安眠药的高效提取、富集,借助GC-MS即可实现快速检验,具有绿色、高效、简便、廉价等优势。

【Abstract】 A dispersive liquid-liquid microextraction(DLLME) device based on hydrophobic porous polydimethylsiloxane sponge(PDMS-Sponge) was established to achieve rapid and efficient extraction of 12 common benzodiazepines drugs in urine. Direct injection test and identification method were achieved with the assistance of gas chromatography-mass spectrometry(GC-MS). The preparation of hydrophobic porous organic PDMS sponge material was achieved through the framework provided by sugar cubes. Fourier transforminfrared spectrometer and scanning electron microscopy were used to characterize the microstructure and performance of PDMS-Sponge. The extraction device was completed by combining medical syringes,magnetic stirrers,and rubber plugs. Quantitative analysis using the internal standard method was conducted to investigate the effects of dispersant,pH value,magnetic stirring time,and dispersant dosage on the extraction efficiency of 12 drugs in urine.The results showed that PDMS-Sponge is a hydrophobic porous material, which can be combined with a medical syringe to construct a new dispersive liquid-liquid microextraction device. Using 100μL of dichloromethane as the extractant,50 μL of acetonitrile as the dispersant,a speed of 800 r/min,and magnetic stirring for 1 min can achieve the extraction and enrichment of the analytes. Under optimal conditions,12 common hypnotics in urine have a good linear relationship in the range of 0. 1-10 μg/mL, with correlation coefficients(r2) greater than 0. 99, detection limits of 0. 025-0. 200 μg/mL,and quantitation limits of 0. 050-0. 400 μg/mL. The recoveries at three spiked levels was 64. 4%-112%,and the relative standard deviations was 0. 80%-9. 4%. The newly dispersive liquid-liquid microextraction device can complete the efficient extraction and concentration of hypnotics in urine in a few minutes,and rapid testing can be achieved with the assistance of GC-MS,providing a green,efficient,simple and inexpensive new dispersive liquid-liquid microextraction solution.

【基金】 广州市民生科技攻关专题(2019030009)
  • 【文献出处】 分析测试学报 ,Journal of Instrumental Analysis , 编辑部邮箱 ,2025年03期
  • 【分类号】O657.63;D918
  • 【下载频次】38
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